CN1365271A - Antipers pirant compositions - Google Patents
Antipers pirant compositions Download PDFInfo
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- CN1365271A CN1365271A CN00810971A CN00810971A CN1365271A CN 1365271 A CN1365271 A CN 1365271A CN 00810971 A CN00810971 A CN 00810971A CN 00810971 A CN00810971 A CN 00810971A CN 1365271 A CN1365271 A CN 1365271A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q15/00—Anti-perspirants or body deodorants
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/37—Esters of carboxylic acids
Abstract
Antiperspirant compositions herein comprise an antiperspirant active, together with a carrier and a structurant for the carrier which comprises an organic wax having a melting point of from 40 to 90 DEG C of which at least 60 % of the weight of the wax is provided by at least one aliphatic ester satisfying the formula:- CH3-(CH2)n-O-CO-(CH2)m-CH3 in which n is from 9 to 39 and m is from 0 to 35 to form a solid or a soft solid. The compositions can be anhydrous, in the form of a suspension of antiperspirant active, or can comprise aqueous emulsions. The formulations structured by the selected waxes provide lower visible deposits on topical application compared with conventional wax-structured formulations and the waxes are effective at structuring/thickening at a proportion below that in conventional wax-structured formulations.
Description
Invention field
The present invention relates to contain the cosmetic composition of thickening or structuring liquid, be specifically related to contain the sort of compositions of antiperspirant and/or deodorant activating agent.
Background and prior art
Many in the world geographic people are extensive use of the Antipers pirant compositions of local coating, and said composition can make user avoid or farthest alleviate the wet speckle at visible wet speckle (wet patch), especially axillary fossa position on their skin.Use different applicators to use the antiperspirant preparation according to the individual's of consumer hobby, these applicators comprise aerosol type applicator, bobbin type applicator, pump formula spray applicator, bar type applicator and mushroom-shaped applicator.Certain areas in the world, rod are popular especially.Term " rod " is meant the solid matter bar traditionally, and described is contained in the proportion container and its complete, promptly firm rod of maintenance in application usually.When the part of firm rod was smeared skin surface, the film transfer of described stick compositions was to skin surface.Though rod has the outward appearance of solid articles, the described material that forms rod has the structure liquid phase usually, and the thin film of described like this compositions is transferred on its another surface that contacts from rod easily.
Since nearer, term " rod " has been applied to soft solid, these soft solids have tangible solid form in storage process, flow but produce under slight extruding or shearing, and so in use they can be expressed on the surface to be prepared burden by a hole or a plurality of hole.After extruding under so non-shearing/low-stress, soft solid keeps their 30 seconds of profile at least, if but stand high shear or when heavily stressed, their structure will be destroyed and after shearing/stress was removed, the structure of a no more than small part can be restored in about 24 hours.
Usually the antiperspirant rod has three types, i.e. suspension rod, latex rod and solution rod.The suspension rod comprises the granule hidroschesis activating agent material that is suspended in the structured supports.The latex rod contains oil phase usually and contains the aqueous-favoring solution of hidroschesis activator solution, and wherein continuous phase is by structuring.In some latex rods, described continuous phase is oil phase.In the solution rod, usually antiperspirant is dissolved in structurized liquid-carrier mutually in.Liquid phase in the solution rod can contain water and/or organic solvent that can be miscible with water.In this three types of rods that can be applicable to hard solid and soft solid compositions.
Many rods adopt natural existence or synthetic wax structuring in the routine, and the object lesson of these waxes comprises stearyl alcohol, chloroflo or siloxane wax.Wax extensively can get, by suitably itself and the concentration in preparation thereof being selected to obtain effectively soft solid or hard solid.Thus, at Cosmetics and Toiletries, 1990, the 105 volumes are described in the article of 75-78 page or leaf as the structurized rod of wax.The cream of wax thickening is described in USP5102656 (Kasat).
Though do not mention the shortcoming of existence in the above referred-to references, but observed and stayed visible white deposits when the structurized compositions of wax will cause on putting on human skin, when carrying out physics when contacting with skin, these deposits also can be transferred on the described clothes, and existing antiperspirant consumer tangible, the ratio that may get more and more shows being sick of the visible deposition thing.Therefore, the antiperspirant industry comprises that the inventor has dropped into a large amount of time and resource to find to improve or overcome the method for consumer to the sedimental sensation of white.
In the natural wax type that exists that is used for or considers to be used for the oily liquid phase of thickening or structuring antiperspirant or deodorant composition, animal sources wax comprises that Cera Flava, plant source wax comprise candelilla wax and Brazil wax.Each of these waxes generally includes the mixture of following material: a) ester, generally include moieties with at least 8 carbon atoms derived from fatty acid or aliphatic alcohol, and/or aromatic hydrocarbon part, b) non-esterified fatty acid, c) non-esterified aliphatic alcohol, d) on-gaseous hydrocarbon and e) resin.The wax components in proportions can be decided according to concrete selected wax, but not quite relevant with its production area and productive life.
Cause existing various shortcomings owing to having mixed naturally occurring wax (especially comprising Cera Flava), for example produce qualitative different shortcoming and owing to the shortcoming that in wax mixture, exists non-esterified acid and/or alcohol to produce owing to the difference of the natural composition of these waxes.Therefore, in numerous open source literatures, before mixing some waxes in the cosmetic formulations, they are carried out chemical treatment to improve their ester content.
For example, in USP5176902 by adopt C1-60 list or polyhydroxy-alcohol with all be present in naturally occurring C12-60 fatty acid in the wax convert to they separately ester and with described wax esterization, mix these waxes subsequently and obtain chromatic cosmetic stick.In the open 58-092605 of Japanese unexamined patent, the mellisic production of modification has been described, wherein with the free acid esterification.Show that described product makes pigment have excellent dispersibility in as the massage cream.In EPA319062 and USP4948584, Koster Keunen has described a kind of by removing the mellisic method of free acid modification.The product of gained has the performance of self emulsifying.Neither ones were mentioned the visible white residue of the antiperspirant or the deodorant composition of structuring or multiviscosisty during these were open, did not also mention subsequently how improving or solving described problem.
Yet the subject matter of mixing wax in preparation usually is that structuring or multiviscosisty carrier fluid form a kind of hard or pliable solid.Preferably determine to have the wax of the performance of excellent structuring or multiviscosisty carrier fluid.For example, only need the wax of fraction to reach required multiviscosisty or structuring degree, the choice that has increased the cosmetic composition Producer thus changes remaining composition.In addition, it is relevant with the sedimental observability on skin at least that the inventor recognizes that present deducibility goes out wax, so their conclusion that draws is that the sedimental degree that then can see of still less wax will be few more if desired.
In WO 98/09609, describe the Cera Flava multiviscosisty or the structurized cosmetic composition of use siliconeization (polysiliconyl) modification and in WO 98/09712, described use hexanediol-docosyl Cera Flava multiviscosisty or structurized cosmetic composition.But the inventor is by the research to the preparation that contains them, finds that the Cera Flava derivant changes the thickening of antiperspirant or deodorant carrier fluid or the structurized ability character according to modification.Thus, the fatty acid esterification (as producing hexanediol-docosyl Cera Flava) of observing free fatty acid in the Cera Flava of for example silicone modification and the Cera Flava all produces the material with relatively poor structuring ability.So, the modification Cera Flava that can not obtain having excellent structuring ability to mellisic pretreatment.
The rod that a kind of consideration is used for antiperspirant or deodorant application type comprises the latex rod.This rod comprises continuous phase, has wherein disperseed the drop (being commonly referred to decentralized photo) of second kind of liquid phase.Described continuous phase is a wherein class of hydrophobic or aqueous, and decentralized photo is another kind of.Can easily antiperspirant or deodorant activating agent be mixed at aqueous phase.Can be by mixing the wax structural agent with hydrophobic phase structureization, described wax structural agent is for generally being solid material at ambient temperature, but at high temperature, as under 60 to 120 ℃ (according to selected oil with wax and different) melt, dissolve or be distributed in the oil that constitutes hydrophobic phase.When the mixture with wax structural agent and oil is cooled to when being lower than its solidification temperature, described oil phase will solidify.
When preparation latex rod, should be taken into account various factors.Some factors wherein are opposings mutually.A primary and important factors relates to described biphase ratio separately.Described antiperspirant salts has limited dissolubility at aqueous phase, and the effect of antiperspirant may be improved along with the increase of water ratio thus.But any raising of water ratio will cause the corresponding minimizing of hydrophobic phase free space in described preparation.Organize olefiant selection in conjunction with it, this will influence the hydrophobic ability that strong support continuous phase is provided mutually, and influence the intensity and the integrity of described rod thus.In addition, it also influences this ability that comprises favourable hydrophobic ingredient mutually.
Wax is generally used for or is proposed for the structuring anhydrous formulation, wherein particulate antiperspirant is suspended in the oil phase, but and seldom relates to they are used for structuring latex rod.
The market of product that is used for the oxter is constantly along with the variation of the taste of consumer and life style and develop.A characteristic of the oxter preparation mainly considered of consumer is the visible level at once or subsequently several days after described preparation is applied on the skin in recent years.This is commonly referred to the visible deposition thing.Wax and antiperspirant salts can stay visible deposit on human skin, therefore consider the hobby of present consumer, and hope can reduce or preferably avoid them.When the characteristic that relates to the observability of preparation on any clothes may occur in it and puts on the skin, perhaps betide the transfer that takes place by skin and contacting of clothes subsequently.Equally, hope can reduce or preferably eliminate visible deposition thing on clothes.
Some oil are to be used for distribution antiperspirant or deodorant activating agent on skin, and can produce the effective carrier of visible deposition thing hardly.Various other oil can improve the outward appearance of visible deposition thing, but the free space of this oil in emulsion is subjected to the restriction of the occupied ratio of water.
Can be used for preparing the latex rod oil act on that the front is existing to be described.Another factor relates to the variation of the sense quality of the latex rod that uses different oil preparations.Thus, for example when spreading upon described preparation on the skin, have and high drag resistance or they may demonstrate thin deposit on skin.Be clamminess or feel that they are more greasy when they seem at proportion container or when putting on the skin.
Prior art comprises various the disclosing of the rod that contains aqueous components that disclose.Thus, US-A-4265878 a kind of preparation that is substantially devoid of nonvolatile oil of having given an example for example.Said preparation has high visible deposition thing.US-A-5162378 discloses the emulsion that contains water, but does not contain nonvolatile oil.Resemble ' 878 do not mention the problem relevant and how to address these problems with the preparation that contains nonvolatile oil.US-A-4704271 discloses and has contained a high proportion of dispersion liquid phase, contains the nonvolatile oil of low ratio and the high ethereal oil and the continuous phase of nonvolatile oil ratio, and the structurized preparation of employing stearyl alcohol.Said preparation itself has high-caliber visible deposition thing from its activating agent and structural agent, and can only reduce in limited range.
WO 98/17238 has given an example and has contained the emulsion formulations of nonvolatile oil, and said preparation does not contain volatile siloxane.Therefore, this patent is not mentioned to the restriction of the preparation that requires to contain these two kinds of compositions and in the ratio of selecting and is contained their benefits of two kinds.
Thereby EP-A-0291334 comes the structuring product to avoid use wax by using liquid crystalline phase.Therefore, this patent is not mentioned the structurized measure (provision) that contains the emulsion of volatile siloxane and nonvolatile oil of wax.
EP-A-0281288 a kind of anti-perspiration formulation that adopts the structurized wherein oil phase of stearyl alcohol only to contain the nonvolatile oil of small scale of having given an example.This preparation has high dragging resistance and in fact also have higher visible deposition thing.Therefore, this patent does not mention how addressing these problems.EP-A-0295071 discloses the latex rod that adopts based on the decentralized photo of polyhydroxy-alcohol, and this latex rod also can contain a spot of water.Having given an example, the weight ratio of propylene glycol and water is 4: 1 in decentralized photo.Rod based on the main oleophobic composition of propylene glycol conduct generally has viscosity.
Purpose of the present invention
An object of the present invention is to provide a kind of thickening or structurized Antipers pirant compositions, described Antipers pirant compositions improves or has overcome the shortcoming of visible deposition thing when use has the wax of excellent structuring ability.
Another purpose of some embodiment preferred provides the latex rod that a kind of employing has the wax preparation of excellent structuring ability, and described latex rod has the globality of required sense quality, rod and reduces the combination of visible deposition thing.
The present invention's general introduction
A first aspect of the present invention provides a kind of and contains hidroschesis activating agent, liquid-carrier and be used for the structural agent of described carrier or the Antipers pirant compositions of thickening agent, it is characterized in that: described structural agent or thickening agent contain organic wax of the fusing point with 40 to 90 ℃, and wherein the wax of at least 60% weight satisfies formula :-CH by at least a
3-(CH
2)
n-O-CO-(CH
2)
m-CH
3Aliphatic (acid) ester provide, in the formula n be 9 to 39 and m be 0 to 35.
The wax of choice criteria that meets the chemical composition of special component by employing, and with the major part of its effect wax can be realized adopting the wax of the shortcoming that can improve the visible deposition thing and target that effective structuring ability is provided simultaneously.Detailed description of the present invention
In compositions of the present invention, the main component of described thickening/structurized wax is the ester that meets following general formula:
-CH
3-(CH
2)
n-O-CO-(CH
2)
m-CH
3In the formula n be 9 to 39 and m be 0 to 35.
The selected ester that meets described general formula, or more general ester admixture can comprise (if desired) and can reach 100% wax at most, and the remainder of wax is Cera Flava or one or more its components or is second kind of wax shape structural agent or thickening agent.In many embodiments, the ratio of selected ester accounts at least 70% weight of described wax, preferably at least 80% weight and at least 90% weight most preferably.
The wax of Shi Yonging preferably comprises the free carboxy acid and the hydrocarbon of no more than small scale at least at the most herein.Preferred described wax contains no more than about 4% and the non-esterified carboxylic acid of especially no more than about 2% weight.The content of requirement for height hydrocarbon in described wax is less, and in fact is less than the content in the Cera Flava of routine, specifically is less than 5% weight of described wax, particularly 0 to 2% weight.
In the general formula of described ester, the scope of preferred ester comprise those wherein n be selected from 14 to 24, especially 16 to 20 simultaneously m be selected from 14 to 24,16 to 20 ester especially.In second scope of preferred ester, n is selected from 18 to 38 in described general formula, and m is 0 or 1.Should understand the mixture of the ester of the ester of the ester admixture that can use each preferable range or a kind of preferable range and another kind of preferable range.Mixture comprises the wax and the mixture that contains the wax of n=16 to 20 and m=14 to 20 or preferred 16 to 20 ester of the ester that contains n=14 to 20 and m=14 to 20 easily.
The ester that meets formula given herein can obtain by the esterification of routine, and described esterification is described in the literature is used to have the alcohol of the chain length that is suitable for providing above-mentioned " n " scope and has under the popular response condition of the reaction between the carboxylic acid that is suitable for producing above-mentioned " m " scope chain length and implement.
Wax used herein accounts for 2 to 25% of described composition weight usually.When the hard solid composite of needs, the ratio of wax is at least 5% weight usually, is chosen in usually in 6 to 15% the scope of described composition weight.When needs soft solid compositions, the ratio of wax is usually less than 5% weight, particularly 2 to 4% weight.Should understand when or when using wax near the amount on described border, promptly when 5% ratio is used wax, the material of gained can be soft solid or have hard solid than soft in standard sphere impression test.
The main component of Antipers pirant compositions is the hidroschesis activating agent.Preferred hidroschesis activating agent is with 0.5-60%, and especially 5-30% or 40%, particularly 10%-30 or 35% amount are mixed.
Usually be selected from the astringent active salt with herein hidroschesis activating agent, specifically comprise aluminum salt, zirconates and mixing aluminum-zirconium salt, comprise inorganic salt, organic salt and complex.Preferred astringent salts comprises aluminum, zirconium and aluminum-zirconium halogenide and hydration halogenide, as chloride monohydrate.
Preferred aluminum salt comprises having general formula Al
2(OH)
xQ
yWH
2The hydration aluminum halide of O, Q represents chlorine, bromine or iodine in the formula, and x is 2-5, and x+y=6, and x and y are integer or non-integer, and w represents variable hydration level, it can be 0.Some particularly preferred hydration halide salts comprise activatory aluminium chlorohydrate, and those as describing in EP-A-6739 (Unilever NV etc.) are attached to this paper as a reference with the content in this patent specification.Activatory salt keeps their enhanced activity and is advantageously used in anhydrous basically preparation, does not promptly contain in the preparation of tangible water.Some activatory salt also can keep their enhanced activity in aqueous compositions.
The zirconates that uses as required in can Antipers pirant compositions herein can be represented with following empirical formula: ZrO (OH)
2n-nzB
zWH
2O, z is integer or the non-integer of 0.9-2.0 in the formula, n represents the quantivalence of B, the value of 2-nz is at least 0, B is selected from halogen anion (comprising the chlorine anion), sulfamic acid root, sulfate radical and their mixture, expresses possibility with w the degree of hydration takes place, and it can be 0.B represents the chlorine anion in preferred zirconates, and z can change in the scope of 1.5-1.87.In practice, this class zirconates does not use separately usually, and uses with the component of bonded aluminum and zirconio antiperspirant, and described al composition is selected according to the halid formula of above-mentioned hydration usually.Ideal especially salt comprises blended aluminium chlorohydrate-zirconium, and is optional through overactivation.
The formula that will be appreciated that above-mentioned aluminum salt and zirconates is empirical formula and can is to have the water of coordination of varying number and/or chemical compound and polymeric material and the mixture and the complex of bound water.Specifically, the salt of the normal expression of the hydroxide salt of zirconium with different hydroxy number.
Can advantageously use antiperspirant complex in the present invention based on above-mentioned astringent aluminum salt, zirconates and aluminum/zirconates.Preferred hydration aluminum halide and/or hydration zirconium chloride material are complexation.Described complex uses carboxylic acid or carboxylate radical, preferably aminoacid usually.The amino acid whose example that is fit to comprises dl-tryptophan, dl-beta-phenyl alanine (aniline), dl-valine, dl-methionine and Beta-alanine, preferably has formula CH
3(NH
2) CO
2The glycine of H.
The most desirable combination and aminoacid such as the bonded complex of glycine that is to use hydration aluminum halide and hydration zirconium chloride is as those disclosed in US-A-3792068 (Luedders etc.).Usually some this class Al/Zr complex is called ZAG in the literature.The ZAG activating agent contains aluminum, zirconium and chlorine anion usually, and wherein the ratio of Al/Zr is 2-10, particularly 2-6, (Al-Zr)/and the ratio of Cl is the aminoacid of 2.1-0.9 and various amounts, particularly glycine.The preferred activating agent of this class can derive from Westwood, Summit and Reheis.
In some preparations, the activatory ZAG complex of preferred especially use, this complex can be by the preparation of disclosed method in USP 5486347 (Callaghan etc.).
Other operable activating agent comprises for example the aluminum salt and the astringent titanium salt of those aluctyl .s of describing, borate crosslinked in GB 2299506A.And other activating agents comprise chlorlinergenics, antihistamines and antiandrenerics.
The ratio of solid hidroschesis salt generally includes weight and any chelating agent that can exist of any water in the hydration in compositions.But when antiperspirant salts was dissolved in the solution, its weight did not comprise the water of any existence.
In some embodiments of the present invention, described antiperspirant salts is used with particle form herein, is not specifically using in the property of water-bearing or the aqueous-favoring compositions.This based composition is called anhydrous or substantially anhydrous compositions easily.As when using conventional pouring procedure to fill conventional tube, the size of the antiperspirant salts in this based composition is generally 1 to 200 μ m, and mean diameter is generally 3 to 20 μ m.Also can consider bigger and less mean diameter, as 20 to 50 μ m or 0.1 to 3 μ m.
In other embodiment, described hidroschesis activating agent can the solution form use, and for example wherein said compositions contains polar phase (comprising the solvent that water and/or water soluble mix usually).In this class embodiment, the concentration of (in disperseing polar phase) hidroschesis activating agent is generally 3-60% (only based on described polar phase meter) in solution, and particularly 10% or 20% to reaching as high as 55% or 60% (counting mutually based on this).
The third main component of described compositions is a liquid-carrier, and common ratio accounts for 30% to 95% of described compositions, particularly 40 to 90%.
Mixing carrier in the compositions herein comprises one or more be liquid under described compositions serviceability temperature, and can be extruded solid material under this serviceability temperature, to provide firmly maybe by structural agent gelling or structuring, wherein said serviceability temperature is generally the ambient temperature of inhabitation, usually be lower than 40 ℃, be lower than 30 ℃ in many cases and also be at least 15 ℃ usually.Described carrier can be hydrophobic carrier or can be hydrophobe and the mixture of hydrophile, and the latter exists with the form of emulsion usually.What need especially is that herein carrier contains enough hydrophobic substances to obtain continuous phase, wherein can disperse discontinuous aqueous favoring or granule phase.But the of the present invention pair of gellant system is particularly suitable for gelling hydrophobic medium and the dispersive oil phase of structuring also, as long as this exists mutually.
Described hydrophobic carrier liquid can have certain volatility or contain volatile ingredient, but the vapour pressure under 25 ℃ is usually less than 4kPa, thus these materials to can be described as be oil or oily mixture.More particularly, the hydrophobic carrier liquid of wishing at least 80% weight material that should be no more than 4kPa by the steam pressure value under 25 ℃ is formed.
In order to promote good sense quality when using described preparation, a class carrier that needs especially is hydrophobic carrier and comprises liquid silicon herein.The siloxane carrier of preferred major part at least is by at least a volatility polysiloxane, and promptly (about 20 ℃ to 25 ℃) have the liquid substance formation that can survey steam pressure under environmental condition.Usually volatile siloxane is 1 or 10Pa-2kPa 25 ℃ vapour pressure.The volatility polysiloxane can be linear or ring-type or their mixture.Preferred annular siloxane comprises polydimethylsiloxane, and particularly those contain 3-9 silicon atom, more preferably no more than 7 silicon atoms, and the polydimethylsiloxane of 4-6 silicon atom most preferably, or often be called as cyclomethicone.Preferred linear siloxanes comprises the polydimethylsiloxane that contains 3-9 silicon atom.Common described volatile siloxane self shows and is lower than 1 * 10
-5m
2/ s (10 centistoke) particularly is higher than 1 * 10
-7m
2The viscosity of/s (0.1 centistoke), linear siloxanes shows usually and is lower than 5 * 10
-6m
2The viscosity of/s (5 centistoke).Described volatile siloxane also can contain the linear or annular siloxane of branching, as above-mentioned by one or more side-O-Si (CH
3)
3Linear or the annular siloxane that-Ji replaces.The example of commodity silicone oil comprises that the rank trade mark from Dow Corning Corporation is 344,345,244,245 and 246 oil, from the Silicone7207 of Union Carbide Corporation and Silicone 7158 and from General Electric[US] SF1202.The ratio that volatile siloxane is present in the described compositions usually reaches as high as 80%, and particularly 10 to 70%, be 20 to 60% in many cases.
The hydrophobic carrier that uses in compositions of the present invention can be optionally or is contained non-volatile silicone oil in addition, and it comprises poly-alkylsiloxane, polyoxyethylene alkyl aryl radical siloxane and polyether siloxane copolymer.These non-volatile silicone oils can suitably be selected from poly dimethyl silicone and poly dimethyl silicone copolyol.The commodity non-volatile silicone oil comprises Dow Corning 556 and DowCorning 200 series (viscosity with at least 50 centistokes).Non-volatile siloxane exists with about 30%, preferred 1 to 15% the amount of no more than described composition weight usually.In many cases, when having non-volatile silicone oil, the weight ratio of itself and volatile silicone oils is 1: 3-1: 40.
Except or replace liquid silicon, can in compositions of the present invention, mix not siliceous hydrophobic organic carrier, hydrophobic carrier liquid as 0 to 100%.This not siliceous hydrophobic organic carrier material can comprise liquid aliphatic hydrocarbon such as mineral oil or Parleam, often selects them to have lower viscosity.Other example of liquid hydrocarbon is poly decene and has the isomery paraffin that at least 10 carbon atoms also reach as high as 30 carbon atoms usually.
Other hydrophobic carrier that is fit to comprises liquid aliphatic ester or aromatic ester, as the part of water immiscibility carrier, it is desirable to be no more than the water immiscibility carrier weight 20%, be lower than 10% in many cases.
The aliphatic (acid) ester that is fit to contains at least one chain alkyl, as derived from by C
8-C
22Alkanoic acid or C
6-C
10The C of chain docosandioic acid esterification
1-C
20The ester of alkanol.Preference chain alkanol and acid moieties or their mixture are lower than 20 ℃ fusing point thereby they are had.Suitable ester comprises isopropyl myristate, tetradecanoic acid dodecyl ester, hexadecanoic acid isopropyl ester, Dermol DIPS and diisopropyl adipate.
Preferred fusing point is lower than 20 ℃ the liquid aromatic ester that is fit to and comprises benzoic acid fat Arrcostab.The example of this class ester comprises suitable benzoic acid C
8-C
18Arrcostab or their mixture.
Other example of the hydrophobic carrier that is fit to comprises the liquid aliphatic ether derived from least a aliphatic alcohol, for example lower alkyl ether (as the PPG-14 butyl ether) of myristyl ether derivant (as the PPG-3 myristyl ether) or poly-dihydric alcohol.Ratio at ether described in the preparation of the present invention is generally 0 to 40% w/w, is in particular 1 to 30% w/w in some preparations.
And other hydrophobic carriers that are fit to are the aliphatic alcohol that contains at least 10 carbon atoms of liquid under being included in 20 ℃.These pure examples comprise branched-chain alcoho, as ethyl hexanol, octyldodecanol and isooctadecanol.Ratio at alcohol described in the preparation of the present invention is generally 0 to 40% w/w, is in particular 1 to 30% w/w.
The toatl proportion of total non-silicone hydrophobic carrier account for usually described vehicle weight 0 to 80% and be in particular 5 to 70%.Can use the mixture of hydrophobic non-silicone organic carrier.Do not have the organic hydrophobic liquid of silicon if use contains oxygen, then require the amount of described liquid to be no more than 70% of hydrophobic carrier weight.The hydrophobic phase of low ratio, it also is possible reaching as high as 20,30 or 35% gross weight.
Can suitably use the mixture by any weight ratio of siloxanes and non-silicone carrier herein, in many test implementation schemes, described ratio is 20: 1 to 1: 20.
Carrier of Shi Yonging or carrier mixture can be and be anhydrous in many effective composition in the present invention, promptly do not contain free water, and this can realize by only adopting one or more hydrophobic carriers.Perhaps, if desired, except above-mentioned those hydrophobic carriers, described compositions also can comprise hydrophilic support, specifically as water and/or mixed organic solvent such as the mixed solvent of alcohols water soluble of water soluble.The compositions that contains hydrophobic and hydrophilic support simultaneously is generally with they wherein a kind of as decentralized photo.
The preparation that contains decentralized photo generally also contains emulsifying surfactant in practice, as anionic, cationic, amphion and/or nonionic surfactant.
In the emulsion herein, describedly comprise that any decentralized photo that is dissolved in material wherein is general to constitute 5 to 80% of described composition weight, reach as high as 65% weight in many cases and in these or other embodiment, preferably be at least 25% weight.The continuous phase that contains structural agent has constituted the remainder of described compositions, as 20 to 95% weight.Emulsion herein contains water-in-oil emulsion usually, and promptly described decentralized photo is an aqueous favoring.When using emulsion, can with described emulsion with before the residual components of described compositions is mixed, in independent step, prepare described emulsion easily.
Mix one or more emulsifying agents in many cases in emulsion, described emulsifying agent is generally nonionic.Usually the ratio that is chosen in emulsifying agent in the described emulsion or emulsifier system (being the mixture of emulsifying agent) is 0.1 to 10% w/w, is 0.25 to 5% w/w in many cases.Most preferably be 0.1 or 0.25% to reaching as high as 3% w/w.Preferably use total HLB value to be 2-10, emulsifying agent or the emulsifier system of preferred 3-8.
Can adopt emulsifier system easily, described system comprises a kind of emulsifying agent and has HLB value and a kind of combination with the HLB value that is lower than desirable value that is higher than required total value.By using this two kinds of emulsifying agents in the proper ratio together, be easy to obtain to promote the weight average HLB value of emulsion formation.
Many suitable emulsifying agents are nonionic ester or ether emulsifying agent, these emulsifying agents contain a polyoxyalkylene part, polyoxyethylene part particularly, usually contain about 2 to 80, special 5 to 60 ethylene oxide units, and/or contain polyol such as glycerol or Sorbitol or other sugar alcohol as hydrophilic segment.Described hydrophilic segment can contain polyoxypropylene.Described emulsifying agent also contains hydrophobic alkyl, alkenyl or aralkyl moiety in addition, contains about 8-50 a carbon atom, a particularly 10-30 carbon atom usually.Described hydrophobic part can be linear or branched, and is normally saturated although can be undersaturated, and optional be fluorizated.Hydrophobic part can contain the mixture of different chain length, and for example those are derived from the mixture of the material of Adeps Bovis seu Bubali, Adeps Sus domestica, Petiolus Trachycarpi oil, Oleum Helianthi or soybean oil.These nonionic surfactant also can be derived from polyol such as glycerol or Sorbitol or other sugar alcohol.The example of emulsifying agent comprise ceteareth-10 to-25, cetech-10-25, steareth-10-25 and PEG-15-25 stearate or isostearate.Other example that is fit to comprise C10-C20 fatty acid list-, two or triglyceride.Other example comprises the C18-C22 fatty alcohol ether of poly(ethylene oxide) (8-12 EO).
Usually the example of coemulsifier that has the low HLB value of 2-is polyhydric alcohol such as the fatty-acid monoester of glycerol or Sorbitol, erithritol or trimethylolpropane or possible diester.Fats portion is generally C14-C22, and is saturated in many cases, comprises cetyl, octadecyl, eicosyl and docosyl.Example comprises Palmic acid or stearic monoglyceride, myristic acid, Palmic acid or stearic Sorbitol list or diester, and stearic trimethylolpropane monoesters.
An ideal especially class emulsifying agent comprises polydimethylsiloxanecopolymer copolymer, i.e. the dimethyl polysiloxane of polyoxyalkylene modification.Polyalkylene oxide groups is generally the copolymer of polyethylene glycol oxide (POE) or polypropylene oxide (POP) or POE and POP.Described copolymer is alkyl-blocked with C1-C12 usually.
The emulsifying agent that is fit to can derive from various commodity, and these commodity comprise Abil
TM, Arlacel
TM, Brij
TM, Cremophor
TM, Dehydrol
TM, Emerest
TM, Lameform
TM, Quest PGPH
TM, Pluronic
TM, Prosorine
TM, Span
TM, Tween
TM, SF1228, DC3225C and Q2-5200.
Described hydrophilic support comprises water usually, and except water or replace water and can comprise that one or more water solublity or water can miscible liquid.The ratio of water is chosen in usually and reaches as high as 60% scope in emulsion of the present invention, and is specially 5% to 40%.Some water can be introduced as the solvent of described hidroschesis activating agent.
One class water solublity or water miscible solvent comprise the short chain single hydroxyl alcohol, as C1-C4, and particularly ethanol or isopropyl alcohol, it can give the ability of preparation deodorant.Another kind of water seeking liquid comprises that preferred fusing point is lower than 40 ℃ or for mixable glycol of water or polyhydric alcohol.The example of binary or polyhydric alcohol comprises ethylene glycol, 1,2-propylene glycol, 1,3 butylene glycol, hexanediol, diethylene glycol, dipropylene glycol, cellosolvo, diethylene glycol monomethyl ether and triethylene glycol monomethyl ether.Especially preferably contain glycerol or Sorbitol and relevant can be as the polyhydric alcohol of the chemical compound of wetting agent.Single, two or the ratio of polyhydric alcohol in described preparation reaches as high as 15%, be 0.5 to 12% in many cases, reach as high as about 5% and preferably approximately 0.2 to 3% easily.
In some embodiment preferred of the present invention, described compositions is the form of emulsion, and wherein continuous phase contains 10 to 35% volatile silicone oils, and 5 to 15% non-volatile hydrophobic oils.Described decentralized photo accounts for 40 to 75%, described antiperspirant or deodorant activating agent account for 1 to 35%, described wax structural agent accounts for 7 to 25%, described emulsifying agent accounts for 0.1 to 10%, and preferred described compositions contains and reaches as high as 5% insoluble granule material, and wherein said percetage by weight is calculated based on the weight of described compositions.
By adopting the compositions of the composition of in above-mentioned specified scope, selecting in preferred embodiments, can prepare bonded antiperspirant or deodorant latex rod: avoid or improve the visible deposition thing, avoid or improve thin deposit, avoid or improve dragging resistance, avoid or improving viscosity and improvement or keep the acceptable sliding sense of consumer (glide), continue the acceptable excellent hardness of enjoyment simultaneously with following two or more excellent properties.In other words, can go out rod, wherein adopt wax of the present invention to carry out structuring and it has the characteristic that many consumers are liked by emulsion preparation.
In described embodiment preferred, carefully select the relative scale of water and oil phase so that obtain the balance of character.The ratio of described water is generally in the scope of 30 to 70% weight, and described percetage by weight has been considered anyly to be dissolved in the water or to form single-phase and material that exist with water.The no more than described composition weight of preferred described water-phase component 65% and be 45 to 60% weight in many ideal embodiments.Many favourable compositionss contain the water of 50% weight.
In described preferred embodiment the water content of water account for usually this phase weight 40 to 75%, and common no more than 65% weight.In practice, the ratio of water accounts for 20 to 40% weight of described composition weight usually, is 24 to 36% weight in many cases.
But the water that has vast scale in emulsion usually prospective consumers will be felt wet and cool characteristic.But surprisingly, the latex rod of the preferred embodiment of the invention is similar to those characteristics of anhydrous rod sensuously.
Except water, the water in emulsion contains antiperspirant or water solublity deodorant usually.The ratio of these materials is at least 0.5% weight usually, is at least 2% weight usually, is at least 5% weight in many cases and reaches as high as 30% weight under same case or other situations.The amount of preferred described antiperspirant is at least 10% weight and is 20 to 25% weight in many preferred emulsions in described embodiment preferred.
Can in described preferred emulsions embodiment, mix a spot of C ideally
2-C
6Dihydroxy or aliphatic polyhydroxy alcohol for example mix with half ratio of the water weight that reaches as high as described water.Usually, the ratio of described dihydroxy or polyhydroxy-alcohol accounts for 0 to 15% weight of described emulsion, particularly 3 to 12% weight.The example of preferred dihydroxy or polyhydroxy-alcohol comprises propylene glycol, glycerol or Sorbitol.Only mix a spot of this class alcohol by restriction, can further limit the degree that occurs from the degree of the cold of described water and evaporation and the visible deposition thing followed, and described compositions does not have uncomfortable being clamminess or other negative sense qualities, as adopt in the emulsion this compounds as described in the main sense quality that fluid composition produced of oleophobic phase.Some particularly preferred emulsions contain the glycerol of 3 to 10% weight.
Although being described emulsion, a benefit of emulsion of the present invention do not have tangible refrigerant sense, can control the algefacient degree by the volatility monohydroxy aliphatic alcohol (as ethanol or isopropyl alcohol) that mixes selection percentage, for example selection percentage is for reaching as high as 5% weight, as at least 0.1% weight.But many particularly preferred preparations do not contain volatile alcohol in the preferred embodiment type.
The hydrophobic carrier liquid that uses in the described preferred embodiment of emulsion of the present invention comprises the mixture of volatile silicone oils and nonvolatile oil, carries out two kinds of components in proportions within the limits prescribed and selects.
In described preferred embodiment, the ratio of preferred volatile silicone oils is not higher than 25% weight and is generally 10 to 20% weight.The ratio of preferred nonvolatile oil is at least 8% weight, no more than in many cases 12% weight.Require not only to consider the absolute ratio of oil in described emulsion, but also should be taken into account their relative scale.The weight ratio of preferred existing volatile silicone oils and nonvolatile oil is at least 1: 1, particularly at least 5: 4.Preferred this ratio is not higher than 3: 1 and more preferably no higher than 2: 1.By carefully considering the absolute ratio of described ratio and described volatile silicone and nonvolatile oil, described emulsion can be reduced the visible deposition thing, avoid excessive simultaneously and drag resistance and oily benefit combines.
Also require to consider they and the material that produces the visible deposition thing, as the ratio of any astringent salts (as antiperspirant salts) and/or wax structural agent.The weight ratio that preferably is chosen in antiperspirant salt pair nonvolatile oil in the described embodiment preferred is 1: 1 to 4: 1 and is in particular 2: 1 to 10: 3, and the absolute ratio that keeps described nonvolatile oil simultaneously is in the scope of aforementioned proportion.
At the nonvolatile oil of selecting to be used for described preferred embodiment, preferably consider above-mentioned various nonvolatile oil, specifically comprise non-volatile silicone oil, liquid aliphatic hydrocarbon and aromatic ester.Can consider to be used to low melt wax (having the wax that reaches as high as 65 ℃ of fusing points) that part involatile constituent (for example reaching as high as the composition of 30% weight) is provided but may be at least the aliphatic (acid) ester that high melting-point wax (for example those have at least 70 ℃ or more dystectic wax) provides other nonvolatile oils of major part can contain at least one chain alkyl, as derived from adopting C as those
8-C
22Alkanoic acid or C
6-C
10The C of chain docosandioic acid esterification
1-C
20The ester of alkanol.Preference chain alkanol and acid moieties or their mixture have them and are lower than 20 ℃ fusing point.The ester that is fit to comprises isopropyl myristate, tetradecylic acid lauryl, isopropyl palmitate, Dermol DIPS and diisopropyl adipate.The other types of this nonvolatile oil such as aliphatic (acid) ester comprise and contain at least 12 and preferably reach as high as the aliphatic alcohol oil of the aliphatic branching of 30 carbon atoms, as isooctadecanol or octyldodecanol with derived from the liquid aliphatic ether of at least one aliphatic alcohol, as the lower alkyl ether (as the PPG-14 butyl ether) of myristyl ether derivant (as the PPG-3 myristyl ether) or poly-dihydric alcohol.
Requirement preferably reaches as high as the ratio, particularly 1 to 5% weight of 5% weight at the present composition, particularly comprise the graininess insoluble substance of at least a small particle diameter in emulsion.This insoluble substance can be inorganic matter, as Talcum, Silicon stone or clay in small, broken bits.Perhaps, described material can be the hydrocarbon solid of fine granularity, as polyethylene in small, broken bits.The existence of these compositions can improve the sliding sense of described rod.In suspension formulation, these materials can be added in any graininess antiperspirant salts.
Optional member in the present composition can comprise that concentration for example reaches as high as the disinfectant of about 10% w/w.The deodorant activating agent that is fit to can contain hidroschesis slaine, deodorant spice (deoperfume) and/or the antibacterial of effective deodorant concentration, specifically comprise the bactericide such as the chloro aromatic compounds that contain Biguanide derivative, this class material such as the IgasanDP300 that specifically can mention
TM, Triclosan
TM, Tricloban
TMAnd Chlorhexidine.Also having a class is the deodorant that contains Guanoctine, is Cosmosil as trade mark
TMCommodity.
Other optional member comprises eluant (wash-off agent), exists with the amount that reaches as high as 10% w/w usually, to help removing described preparation from skin or clothes.This class eluant is generally non-ionic surface active agent, as contains C
8-C
22The ester of moieties and hydrophilic segment or ether, described hydrophilic segment can contain polyalkylene oxide groups (POE or POP) and/or polyhydric alcohol.
Except described ester (main structural agent), the another kind of optional components of described preparation comprises one or more supplementary structure agent.The amount of this class supplementary structure agent often is 0 in preparation, and is no more than 15% of preparation usually.Usually be no more than the amount of primary structure agent.Will be appreciated that in the emulsion of many embodiment preferred this class supplementary structure agent can not exist or not need.
The supplementary structure agent that can use herein is can right and wrong polymeric or polymeric.Non-polymeric structural agent is sometimes referred to as gellant, can be selected from fatty acid or its salt, as stearic acid or sodium stearate or 12-hydroxy stearic acid.Other gellant that is fit to can comprise the dibenzylidene sugar alcohol, as dibenzylidene sorbitol.Other gellant that is fit to can comprise lanosterol; the N-acyl amino acid derivative of selecting (comprises ester and amide derivatives; as N-lauroyl glutamate dibutyl amide), consider that this gellant can play a role jointly with hydroxy stearic acid or its ester or amide derivatives.Other gellant comprises two or the amide derivatives of tricarboxylic acid, as alkyl N, and N '-dialkyl group succinamide, dodecyl N for example, N '-dibutyl succinamide.Can use the wax of stearyl alcohol and/or natural plants or animal derived or similar synthetic wax as the supplementary structure agent if desired.
In some embodiments, described supplementary structure agent comprises the candelilla wax of candelilla wax or esterification, and it preferably contains 12 to 36 carbon atoms, contains 16 to 24 carbon atoms especially, can the side carboxyl esterification of described wax be obtained by adopting aliphatic alcohol.The weight ratio convenient and suitable ground of the candelilla wax of main wax and auxiliary candelilla wax or esterification is at least 10: 1, as 3: 1,1: 1 and 1: 3 in many cases for reaching as high as 1: 4.Proved that rod that such combination obtains is than the corresponding hardness height that adopts the preparation that candelilla wax obtains as structural agent separately.
Operable paradigmatic structure agent can comprise the organopolysiloxane elastomer, as polysiloxanes and cross-linking agent or alkyl or the end capped product of gathering (methyl substituted) or poly-(phenyl replaces) siloxanes of alkyl polyoxyalkylene with ethenyl blocking.The polyamide of many structural agents as hydrophobic liquid is also disclosed.If described compositions contains water, then poly-propionyl amide, polyacrylate or polyethers can be in order to this phases of structuring.
The preparation herein that preferably includes described preferred emulsions embodiment does not contain substantially and is generally water-insoluble, and has the solid fatty alcohol of 12 to 30 carbon atoms usually, as stearyl alcohol or docosanol, is lower than 2% weight, especially is lower than 0.5% weight as content.
Compositions herein can be mixed one or more cosmetics additives of considering to be used for antiperspirant solid or soft solid usually.This class cosmetics additive can comprise skin sense improver such as Talcum or the polyethylene in small, broken bits that for example is up to about 10% (w/w); The beneficial skin agent (skin benefit agent) that for example is up to about 5% (w/w) is as allantoin or lipoid; The color material; Usually the skin freshener such as menthol and the menthol derivative that are up to the alcohols that being different from of 2% (w/w) mentioned.Normally used additive is a spice, and the concentration with 0-4% exists usually, and the concentration of spice is 0.25-2% in many preparations.
Compositions described herein can be by the method preparation of conventional supending or emulsion solids or soft solid.
Thus, another aspect of the present invention provides the method for preparing the antiperspirant rod, said method comprising the steps of:
1. mix organic wax with the amount that is enough to multiviscosisty or the described carrier of structuring in the liquid-carrier and can extrude solid or solid to form, described organic wax has 40 to 90 ℃ fusing point, and wherein the wax of at least 60% weight satisfies formula :-CH by at least a
3-(CH
2)
n-O-CO-(CH
2)
m-CH
3Aliphatic (acid) ester provide, in the formula n be 9 to 39 and m be 0 to 35,
2. it is flowable that the described mixture that contains structural agent is become,
3. described liquid-carrier is mixed with the hidroschesis activating agent, step 2 and 3 before step 1, afterwards or carry out containing the mixture of structural agent simultaneously with formation,
4. described flowable mixture is introduced in the proportion container, and
The cooling or make described flowable mixture be cooled to its multiviscosisty or structurized temperature.
A kind of processing sequence that suspends the antiperspirant preparation easily comprises at first described wax is enough being mixed under the high temperature with the described wax of fusion with carrier.Subsequently, can be with granular hidroschesis activating agent and described carrier solution blending, and under the temperature of 5 to 10 ℃ of the freezing pointes that is higher than described blend, be introduced in the described proportion container, as adopt suitable packing method to introduce in the tube and cool off or make it be cooled to ambient temperature.
But a kind of suitable method for preparing emulsion antiperspirant preparation comprises the flowing mixture that at first forms wax and hydrophobic carrier, and is for example the same in the preparation of suspension rod.In introducing hidroschesis activating agent (if desired) mutually, prepare water or aqueous favoring separately because this class activating agent can be distributed in the aqueous solution easily.Preferably described solution is heated to the temperature approaching with oil phase, subsequently each is mixed mutually.Perhaps, can under to described mixture mild heat and under the speed that keeps described mixture temperature, aqueous favoring be incorporated in the oil phase.With suspension rod similar methods described mixture is loaded/cooled off subsequently.
The preferred emulsions embodiment can prepare by the following method:
By mixed volatilization silicone oil at high temperature, nonvolatile oil and wax structural agent form hydrophobic mixture or with described mixture heated to described structural agent fusion or dissolving or be dispersed in temperature in the oil, formed flowable hydrophobic mixture thus,
Form simultaneously or subsequently and contain the water that water solublity or water soluble blend together branchs, in the presence of emulsifying agent described flowable hydrophobic mixture is mixed with water and any insoluble particulate material, formation contains the emulsion of hydrophobic continuous phase and dispersion water thus,
Cooling or make described emulsion be cooled to a certain temperature makes to form solid by the described continuous phase of described structural agent structuring, it is characterized in that described continuous phase contains 10 to 35% volatile silicone oils, 5 to 15% non-volatile hydrophobic oil,
Described decentralized photo accounts for 40 to 75%, described antiperspirant or deodorant activating agent account for 0.5 to 35%, described wax structural agent accounts for 7 to 25%, described emulsifying agent accounts for 0.1 to 10%, and preferred described compositions contains 5% insoluble granule shape material at most, and wherein said percetage by weight is calculated based on the weight of described compositions.
Emulsion formulations described herein can prepare or be used for preparation and contain high interior phase volume by any method of describing so far, as the antiperspirant emulsion of at least 40% weight inner phase.
A kind of suitable method comprises:
1. described wax is incorporated into the amount that is enough to multiviscosisty or structured oil phase in the mixture of described volatile siloxane and nonvolatile oil,
2. make the described mixture that contains structural agent become and can flow under the high temperature, step 1 and 2 can be carried out in order or simultaneously,
3. obtain the aqueous solution of described antiperspirant or deodorant, the optional emulsifying agent that contains,
4. in the presence of emulsifying agent, the flowable mass that will prepare in step 2 and the aqueous solution of step 3 also form emulsion under shear at high temperature,
With described still be that the emulsion of flowable mixture is introduced in the proportion container, and
The cooling or make described emulsion be cooled to its solidified temperature.
In step 2, requirement for height keeps described mixture at selected high temperature and be higher than under 5 to 10 ℃ the temperature of fusing point of wax of peak melting point, is dispersed in fully in the described oil phase up to described wax.
In step 3, easily emulsifying agent is introduced usually and contained the pre-formation solution of described antiperspirant salts, but in other cases, solid antiperspirant can be dissolved in aqueous phase.This step is at high temperature implemented usually or usually described solution is heated to high temperature in step 4 with before described flowable oil phase mixes.Usually described water is heated in 20 ℃ of described oil phase temperature.
In step 4, in the presence of shearing condition and emulsifying agent with described two liquid-phase mixing together.Obtain the drop of decentralized photo like this.This step is implemented under the temperature that remains on the solidification temperature that is higher than preparation, forms according to it, is chosen in usually in about 50 to 70 ℃ scope.
In step 5, but with the flowable emulsion leading-in rod measurer of step 4 (being commonly referred to tube).This can use conventional pouring procedure to implement, and maybe can use as the injection molding technology of describing in PCT application number PCT/EP99/07249 and implement.Equally, the flowable suspension of preparation can be under pressure in the step 3 of suspension scheme, preferably in about 3 ℃ temperature range of the conventional solidification temperature of described preparation in the injecting tube.
In step 6, but pressure will contain the measurer cooling of described flowable emulsion, pass through the cooling duct as conveying, if or for example they in step 5 (or in step 4 of suspension scheme) load (in 3 ℃ of scopes of the conventional solidification temperature of described preparation, operating) by injection molding technology, then can it be cooled off at ambient temperature.
Compositions herein is suitable for the part and is applied on the human skin, and particularly Antipers pirant compositions is applied on the axillary fossa, has reduced visible perspiration thus.
Thus, third aspect present invention provides the method that stops or reduce the human skin perspiration, described method comprises that the Antipers pirant compositions part that will contain hidroschesis activating agent, liquid-carrier and structural agent is applied on the skin, wherein said structural agent contains organic wax of the fusing point with 40 to 90 ℃, and wherein the wax of at least 60% weight satisfies formula :-CH by at least a
3-(CH
2)
n-O-CO-(CH
2)
m-CH
3Aliphatic (acid) ester provide, in the formula n be 9 to 39 and m be 0 to 35.
It is desirable to the part especially and apply described particularly preferred antiperspirant or deodorant emulsion compositions, be those contain continuous phase and 40 to 75% disperse waters compositions, described continuous phase contains 10 to 35% volatile silicone oils, 5 to 15% non-volatile hydrophobic oils, wherein said dispersion water contains 1 to 35% antiperspirant or deodorant activating agent, 7 to 25% wax structural agent, 0.1 to 10% emulsifying agent, preferred 5% the insoluble granule shape material that contains at most, wherein said percetage by weight is calculated based on the weight of described compositions.
The common term of the present invention is described, its specific embodiments will be described more completely, but only be exemplarily to describe.
In preliminary test, following various hydrophobic oils are mixed forming mixture with the various specific wax of 10% weight, and with the mixture heated of gained to high temperature (under this temperature all fusions of wax), and be cooled to ambient temperature subsequently.
Oil-volatile siloxane, Silicone DC 556, polyphenylene methoxyl group siloxanes, isooctadecanol, octyl methoxycinnamate, PPG-14 butyl ether, benzoic acid C
12-15Arrcostab, mineral oil.
Wax-K62, K66, K69, K82H and K82N.
The material of gained is opaque gel entirely, and it can be the softest (soft/hard) to the hardest (stone).
Embodiment 1 to 15 and comparative example C16 to C18
In embodiment 1 to 15 and comparative example C16 to C18, excellent by following universal method preparation according to the suspension of the prescription of in following table 1, summing up:
At first with various oil in conjunction with to obtain carrier mixture.Described wax is incorporated in the described carrier and heated and stirred to 80 ℃ to 100 ℃ and be higher than under the temperature of fusing point of described wax and make its dissolving.Under slowly stirring, the flowable mixture of gained is cooled off subsequently, then under agitation added specific graininess hidroschesis activating agent and it is disperseed fully.When described mixture has reached when being higher than the about 5-10 of its gel point ℃ temperature, be poured in the rod tube, (ambient temperature) makes its cooling and curing in laboratory.
The composition of embodiment is as follows:
(1)vol.sil-DC345(Dow?Corning?Inc)
(2)vol.sil-DC245(Dow?Corning?Inc)
(3) different octyl pelargonate-(Stepan)
(4) PPG-14 butyl ether-Fluid AP (Amercol)
(5) benzoic acid C
12-15Arrcostab-Finsolv TN (Fintex)
(6) poly decene-Silkflo 364 NF (Albermarle)
(7) polydimethylsiloxane-DC 350 (Dow Corning Inc)
(8) PEG-8 distearate-Estol E04DS 3724 (Unichema)
(9) ECDC-cetyl dimethicone copolyol--Abil EM90 (Goldschmidt)
(10) Talcum-Suprafino Talc (Luzenac America Inc)
(11) AZAG-Al/Zr Tetrachlorohydrex glycine complexes (Summit)
(12) 50% aqueous solution (Giulini) of AZCH-hydration pentachloro-Al/Zr
(13) AZG 370-Al/Zr hydration chlorination glycine complexes (Summit)
(14) K62-stearic acid behenic acid C
16-22Arrcostab (C
16-22Alkyl stearatebehenate) wax (62 ℃ of fusing points) (Koster Keunen)
(15) K69-acetic acid C
18-38Alkyl ester type waxes (69 ℃ of fusing points) (Koster Keunen)
(16) K82N-stearic acid behenic acid C
16-22Alkyl ester type waxes (82 ℃ of fusing points) (KosterKeunen)
(17) K82H-stearic acid C
18-38Alkyl ester type waxes (Koster Keunen)
(18) weight ratio of K62/K82H-K62 and K82H is 2: 1
(19) K80P-stearic acid behenic acid C
16-22Alkyl ester type waxes (80 ℃ of fusing points) is (contrast wax) (KosterKeunen)
(20) BW67-stearyl Cera Flava (67 ℃ of fusing points) (Koster Keunen) (contrast wax)
(21) SiBee-silicone Cera Flava (Koster Keunen) (contrast wax)
(22) glycerol-(Aldrich)
(23) Parleam-Panalene-L-14E (Amoco)
(24) the little wick vegetable wax (candellilate wax) (Koster Keunen) of Cetearyl esterification
(25) decyl oleate-Cetiol V
(26) deionized water
(27) hydration five aluminum chloride zirconium-Rezal 67
(28) aluminum zirconium Tetrachlorohydrex GLY-Zirconal 50
(29) particulate polyethylene-Acumist B18 in small, broken bits
(30) spice
(31) Risorex PGIS 22-Lameform TGI
(32) polyglyceryl polyricinoleic acid ester (Polyglyceryl polyricinoleate)-QuestPGPR
(33) Parleam-Fancol 800
(34) Parleam-Fancol 250
(35) 32 carbon diguerbet-Lambent DG 3200
(36) 2-Methylpentadecane-Permethyl 101A
In table 1, SOFT shows that described product penetrates＞soft solid of 50mm for having penetrometer, and its deposit mark does not use available testing equipment.Hereinafter, ball hardness shows that hardness adopts the sphere indentation to test, and penet hardness shows that hardness adopts the penetration depth of pin to measure (as described herein).
The conventional wax structuring (CWS) of contrast rod-employing generally has 0.217N/mm
261 black Pilus Caprae seu Ovis deposit mark in the test of ball hardness and description herein.
Table 1
| The embodiment numbering | ??1 | ??2 | ??3 | ??4 | ??5 | ??6 | ??7 | ??8 | ??9 |
| Composition | Percetage by weight % in the preparation | ||||||||
| vol?sil( 1) | 54.55 | ?48.49 | ?54.55 | ?60.00 | ?54.55 | ?54.55 | ?51.0 | ||
| vol?sil( 2) | ?66.75 | ?49.75 | |||||||
| Different octyl pelargonate ( 3) | 6.75 | ?6.00 | ?6.75 | ||||||
| The PPG-14 butyl ether ( 4) | ?15.0 | ?15.0 | |||||||
| Benzoic acid C 12-15Arrcostab ( 5) | ?6.00 | ||||||||
| Poly decene ( 6) | ?6.75 | ||||||||
| Polydimethylsiloxane ( 7) | ?6.75 | ||||||||
| The PEG-8 distearate ( 8) | |||||||||
| ECDC( 9) | ?4.5 | ?4.5 | |||||||
| Talcum ( 10) | 3.94 | ?3.50 | ?3.94 | ?3.94 | ?3.94 | ||||
| AZAG( 11) | 24.76 | ?22.0 | ?24.76 | ?24.0 | ?24.76 | ?24.76 | ?24.0 | ||
| AZG?370( 13) | ?20.0 | ?20.0 | |||||||
| K62( 14) | 10.0 | ?10.0 | ?10.0 | ?10.0 | ?8.0 | ?10.0 | |||
| K69( 15) | ?10.0 | ||||||||
| K82N( 16) | ?10.0 | ||||||||
| K62/K82H( 18) | ?20.0 | ||||||||
| K80P( 19) | |||||||||
| BW67( 22) | |||||||||
| SiBee( 21) | |||||||||
| Spice | ?0.75 | ?0.75 | |||||||
| Ball hardness (N * 10 -3/mm 2) | 224 | ?183 | ?320 | ?98 | ?201 | ?190 | ?33 | ||
| Penetrate hardness mm | ?16.1 | ?12.1 | |||||||
| The woolen deposit mark of black | 19 | ?16 | ?42 | ?nm | ?29 | ?53 | ?25 | ?39 | ?54 |
Table 1 (continuing)
| The embodiment numbering | ????10 | ????11 | ????12 | ????13 | ????14 | ????15 | ??C16 | ??C17 | ??C18 |
| Composition | Percetage by weight % in the preparation | ||||||||
| vol?sil( 1) | ??54.55 | ??54.55 | ??54.55 | ||||||
| vol?sil( 2) | ????61.75 | ????49.75 | ????51.75 | ????57.75 | ????54.75 | ????59.75 | |||
| Different octyl pelargonate ( 3) | ????5.0 | ??6.75 | ??6.75 | ??6.75 | |||||
| The PPG-14 butyl ether ( 4) | ????5.0 | ????15.0 | ????10.0 | ||||||
| Benzoic acid C 12-15Arrcostab ( 5) | ????15.0 | ????5.0 | |||||||
| Poly decene ( 6) | |||||||||
| Polydimethylsiloxane ( 7) | |||||||||
| The PEG-8 distearate ( 8) | ????4.5 | ????4.5 | ????4.5 | ????4.5 | ????4.5 | ????4.5 | |||
| ECDC( 9) | |||||||||
| Talcum ( 10) | ??3.94 | ??3.94 | ??3.94 | ||||||
| AZAG( 11) | ??24.76 | ??24.76 | ??24.76 | ||||||
| AZG?370( 13) | ????20.0 | ????20.0 | ????20.0 | ????20.0 | ????20.0 | ????20.0 | |||
| K62( 14) | |||||||||
| K69( 15) | ????8.0 | ????10.0 | ????10.0 | ||||||
| K82N( 16) | ????8.0 | ????10.0 | ????10.0 | ||||||
| K62/K82H( 18) | |||||||||
| K80P( 19) | ??10.00 | ||||||||
| BW67( 22) | ??10.00 | ||||||||
| SiBee( 21) | ??10.00 | ||||||||
| Spice | ????0.75 | ????0.75 | ????0.75 | ????0.75 | ????0.75 | ????0.75 | |||
| Ball hardness (N * 10 -3/mm 2) | ??SOFT | ??SOFT | ??SOFT | ||||||
| Penetrate hardness mm | ????19.8 | ????18.8 | ????30.4 | ????13.8 | ????16.5 | ????13.8 | |||
| The woolen deposit mark of black | ????39 | ????29 | ????30 | ????49 | ????35 | ????49 | ??SOFT | ??SOFT | ??SOFT |
By table 1 as seen, all products that obtain in an embodiment have measurable hardness, these are different with the product (C16 to C18) that three kinds of contrast waxes that adopt similar proportion obtain, show wax of the present invention and adopt the Cera Flava of contrast modification to compare performance with excellence at the aspect that structuring Antipers pirant compositions, particularly structuring contain the volatile siloxane preparation.
Should see that product of the present invention and conventional wax structuring (stearyl alcohol) suspension Antipers pirant compositions (CWS) have significantly reduced the generation of white deposits relatively usually.On the other hand, the product of the contrast wax of C16 to C18 is too soft and can't measure white deposits with said method.
In other tests, by trained evaluator group the preparation of embodiment 1 and CWS are contrasted rod and head to head test (head to head test) and make comparisons.A kind of product is applied to an oxter and another kind is applied to another oxter.A left side/right side applied carry out balance.Preparation of the present invention is comparatively favourable, and the visible fractional difference of white deposits is 16 (48/64), has confirmed by described product being applied to resulting result on the non-skin matrix.This difference has the significance on the statistics, has the confidence level greater than 95%.
Embodiment 19 to 31
In these embodiments, the latex rod that has the prescription of summing up in the following table 2 by a kind of or other following universal method preparation:
By preparing oil-continuous phase in the mixture that described wax is incorporated into described oil and emulsifying agent.Described mixture heated to 80 ℃ to 100 ℃ and remain in the about 10 ℃ temperature range of the fusing point that is higher than described wax, is slightly mixed (the low shearing) up to described wax dissolving in the Silverson blender.In embodiment 19 to 23, described mixture is cooled to about 80 ℃.By the active antiperspirant of heating aluminum zirconium in water or the solution in the mixture of water and polyhydric alcohol to the temperature similar to described oil-continuous phase prepare decentralized photo (being also referred to as inner phase).
In embodiment 19 to 23, under the high shear mixing condition, described dissipation of heat is incorporated in the described continuous phase mutually.Reach up to described mixture that just to stop high shear when being higher than about 5 to the 10 ℃ pouring temperature of preparation solidification temperature mixed, be poured in the described rod tube and naturally cool to breadboard ambient temperature.In embodiment 24 to 31, described dissipation of heat slowly is incorporated in the oil phase mutually, improve the mixing rate of described Silverson blender simultaneously gradually.After introducing described decentralized photo fully, mixed described preparation 5 minutes with higher speed once more, mix until reaching the about 10-15 of the solidification temperature that is higher than described preparation ℃ with lower speed subsequently, be poured into this moment in the described rod tube and naturally cool to breadboard ambient temperature.
Table 2
| The embodiment numbering | ??19 | ??20 | ????21 | ????22 | ????23 | ????24 | ????25 | ????26 |
| Composition | Percetage by weight % in preparation | |||||||
| vol?sil( 1) | ??38.92 | ??34.50 | ????30.08 | |||||
| vol?sil( 2) | ????25.65 | ????25.65 | ????21.48 | ????19.49 | ????16.31 | |||
| Different octyl pelargonate ( 3) | ??5.08 | ??4.50 | ????3.92 | ????3.35 | ????3.35 | |||
| Poly decene ( 6) | ????27.15 | ????24.64 | ????20.61 | |||||
| The PPG-14 butyl ether ( 4) | ????5.37 | ????4.87 | ????4.08 | |||||
| ECDC( 9) | ??1.0 | ??1.0 | ????1.0 | ????1.0 | ????1.0 | ????1.0 | ????1.0 | ????1.0 |
| AZCH( 12) | ??50.0 | ??50.0 | ????50.0 | ????50.0 | ????50.0 | ????30.0 | ????30.0 | ????30.0 |
| Glycerol ( 22) | ||||||||
| Water | ||||||||
| K62( 14) | ??5.0 | ????20.0 | ????15.0 | ????20.0 | ????28.0 | |||
| K69( 15) | ????20.0 | |||||||
| K82N( 16) | ??10.0 | |||||||
| K62/K82H( 18) | ????15.0 | |||||||
| Inner phase | ??50 | ??50 | ????50 | ????50 | ????50 | ????30 | ????30 | ????30 |
| Ball hardness (N * 10 -3/mm 2) | ??6 | ??44 | ????37 | ????0.05 | ????0.12 | ????0.25 | ||
| Penetrate hardness mm | ????8.4 | ????8.2 | ????14.4 | ????8.2 | ????3.7 | |||
| The woolen deposit mark of black | ??14 | ??20 | ????21 | ????28 | ????28 | ????25 | ????23 | ????18 |
Table 2 (continuing)
Embodiment 32-36
| The embodiment numbering | ????27 | ????28 | ????29 | ????30 | ????31 | ????32 | ????33 | ????34 | ????35 |
| Composition | Percetage by weight % in preparation | ||||||||
| vol?sil( 1) | |||||||||
| vol?sil( 2) | ????17.5 | ????15.51 | ????13.92 | ????11.54 | ????7.65 | ????9.15 | ????7.96 | ????6.76 | ????3.58 |
| Different octyl pelargonate ( 3) | |||||||||
| Poly decene ( 6) | ????22.12 | ????19.61 | ????17.60 | ????14.58 | ????9.55 | ????11.56 | ????10.05 | ????8.55 | ????4.52 |
| The PPG-14 butyl ether ( 4) | ????4.38 | ????3.88 | ????3.48 | ????2.88 | ????1.89 | ????2.29 | ????1.99 | ????1.69 | ????0.90 |
| ?ECDC( 9) | ????1.0 | ????1.0 | ????1.0 | ????1.0 | ????1.0 | ????1.0 | ????1.0 | ????1.0 | ????1.0 |
| ?AZCH( 12) | ????40.0 | ????40.0 | ????40.0 | ????40.0 | ????40.0 | ????40.0 | ????40.0 | ????40.0 | ????40.0 |
| Glycerol ( 22) | ????5.0 | ????10.0 | ????10.0 | ????15.0 | ????15.0 | ????5.0 | |||
| Water | ????5.0 | ????10.0 | ????10.0 | ????15.0 | ????15.0 | ????15.0 | |||
| ?K62( 14) | ????15 | ????20 | ????24 | ????20.0 | ????20.0 | ????16.0 | ????9.0 | ????12.0 | ????20.0 |
| ?K69( 15) | |||||||||
| ?K82N( 16) | |||||||||
| ?K62/K82H( 18) | |||||||||
| Inner phase | ????40 | ????40 | ????40 | ????50 | ????60 | ????60 | ????70 | ????70 | ????70 |
| Ball hardness (N * 10 -3/mm 2) | ????0.05 | ????0.16 | ????0.18 | ????0.21 | ????0.21 | ????0.10 | ????0.04 | ????0.09 | ????0.20 |
| Penetrate hardness mm | ????13.6 | ????5.8 | ????5.1 | ????4.5 | ????5.0 | ????7.7 | ????12.4 | ????12.3 | ????4.8 |
| The woolen deposit mark of black | ????23 | ????24 | ????17 | ????19 | ????17 | ????22 | ????18 | ????16 | ????18 |
In these embodiments, sum up as following table 3 and the preparation that contains a small amount of structural agent prepares by following universal method:
In the Silverson blender,, be heated to about 70 ℃ simultaneously with speed mixed volatilization siloxanes, oil and the wax structural agent of 3000rpm.Under identical condition, introduce particulate matter, reduce agitator speed subsequently to 1000rpm and cool off described mixture simultaneously to about 57 ℃.Subsequently, do not carrying out cooling off described mixture under the condition of stirring again to ambient temperature.
Table 3
| The embodiment numbering | ??36 | ??37 | ??38 | ??39 | ??40 | ??41 |
| Composition | Percetage by weight % in the preparation | |||||
| vol?sil( 2) | ??61.5 | ??65.75 | ??61.5 | ??65.75 | ??61.5 | ??65.75 |
| Different octyl pelargonate ( 3) | ??7.25 | |||||
| Benzoic acid C 12-15Arrcostab ( 5) | ??7.25 | |||||
| The PPG-14 butyl ether ( 4) | ??7.25 | |||||
| Poly decene ( 6) | ??7.25 | |||||
| Polydimethylsiloxane ( 7) | ??7.25 | |||||
| Polyisobutylene ( 23) | ??7.25 | |||||
| Talcum ( 10) | ??4.25 | ??4.25 | ??4.25 | |||
| AZAG( 11) | ??24.0 | ??24.0 | ??24.0 | ??24.0 | ??24.0 | ??24.0 |
| K62( 14) | ??3.0 | ??3.0 | ??3.0 | ??3.0 | ??3.0 | ??3.0 |
Zhi Bei preparation all is the form of soft solid in these embodiments.
Embodiment 42 to 44
In these embodiments, repeat embodiment 1, but adopt Cera Flava ester and esterification candelilla wax in conjunction with replacing adopting separately the Cera Flava ester, the wherein ratio of Cera Flava ester and esterification candelilla wax such as following table 4 are also listed the character of gained preparation in the table.
Table 4
| The embodiment numbering | ????42 | ????43 | ????44 |
| Composition | % in preparation (w/w) | ||
| K62( 14) | ????2.5 | ????5.0 | ????7.5 |
| The candelilla wax of esterification ( 24) | ????7.5 | ????5.0 | ????2.5 |
| The non-wax component of embodiment 10 | ????90 | ????90 | ????90 |
| Character | |||
| Penetrometer hardness mm | ????11.7 | ????19.7 | ????7.5 |
| The woolen deposit mark of black | ????53 | ????56 | ????60 |
The various character of summing up described rod in last table are to obtain and will the results are summarized in this table by methods analyst described below.Assessment is to carry out after at least 24 hours in that the gained rod is stored in the laboratory environment temperature.
The material of gained is opaque gel, and it is soft/hard (the softest) to the utmost point hard (the hardest).Embodiment 46 to 51 and comparative example C45 to C52
The preparation of embodiment 46 to 51 and comparative example C45 prepares by following universal method:
By preparing oil-continuous phase in the mixture that described wax is incorporated into described oil and emulsifying agent.Described mixture heated to 80 ℃ to 100 ℃, is remained in the about 10 ℃ temperature range of the fusing point that is higher than described wax then, in the Silverson blender, slightly mix (the low shearing) up to described wax dissolving.Described mixture is cooled to about 80 ℃.By the active antiperspirant of heating aluminum zirconium in water or the solution in the mixture of water and polyhydric alcohol to the temperature close with described oil-continuous phase prepare decentralized photo (being also referred to as inner phase).
Described dissipation of heat slowly is incorporated in the oil phase mutually, improves the mixing velocity of described Silverson blender simultaneously gradually.After introducing described decentralized photo fully, mixed described preparation 5 minutes with more speed once more, mix until reaching the about 10-15 of the solidification temperature that is higher than described preparation ℃ with lower speed subsequently, be poured into this moment in the described rod tube and naturally cool to breadboard ambient temperature.
Except comparative example C52 (adopting the structurized suspension antiperspirant of conventional wax rod), gained preparation and characteristic thereof are summarized in the following table 5.Term u/a represents the oxter.
Table 5
| Composition | ???C45 | ????46 | ????47 | ???48 | ??49 | ???50 | ????51 | ?C52 |
| ????vol?sil1 | ???30.65 | ????12.6 | ????12.6 | ???12.6 | ??18.5 | ???12.6 | ????12.6 | |
| Oil 4 | ???3.35 | ????--- | ????--- | ????--- | ??--- | ???--- | ????--- | |
| Oil 5 | ???--- | ????8.4 | ????8.4 | ????8.4 | ??12.5 | ???--- | ????--- | |
| Oil 25 | ???--- | ????--- | ????--- | ????--- | ??--- | ???8.4 | ????--- | |
| Oil 23 | ???--- | ????--- | ????--- | ????--- | ??--- | ???--- | ????8.4 | |
| Emulsifying agent 9 | ???1.0 | ????1.0 | ????1.0 | ????1.0 | ??1.0 | ???1.0 | ????1.0 | |
| Water 26 | ???--- | ????--- | ????4.5 | ????4.5 | ??4.5 | ???4.5 | ????4.5 | |
| Glycerol 22 | ???--- | ????4.5 | ????--- | ????--- | ??--- | ???--- | ????--- | |
| Talcum 10 | ???--- | ????--- | ????--- | ????2.0 | ??2.0 | ???2.0 | ????2.0 | |
| ????AZCH?27 | ???--- | ????58.0 | ????58.0 | ????58.0 | ??--- | ???58.0 | ????58.0 | |
| ????AZCH28 | ??50.0 | ????--- | ????--- | ????--- | ??48.0 | ???--- | ????--- | |
| Wax 14 | ??15.0 | ????12.5 | ????12.5 | ????12.5 | ??12.5 | ???12.5 | ????12.5 | |
| ????PE?29 | ???--- | ????2.0 | ????2.0 | ????--- | ??--- | ???--- | ????--- | |
| Oil 30 | ???--- | ????1.0 | ????1.0 | ????1.0 | ??1.0 | ???1.0 | ????1.0 |
Table 5 (continuing)
Embodiment 53 to 55
| Feature | ||||||||
| Hardness (mm) | ??8.4 | ??5.9 | ??5.7 | ??5.7 | ???7.4 | ???4.1 | ???6.1 | ???7.3 |
| Aries hair (0h) | ??13 | ??18 | ??18 | ??20 | ???36 | |||
| Pilus Caprae seu Ovis (24h) | ??72 | ??27 | ??32 | ??23 | ???87 | |||
| The critical sensory data | ||||||||
| Refrigerant | ??10 | ??30 | ??32 | ??41 | ???14 | |||
| White point (flakes) | ??17 | ??1 | ??9 | ??10 | ???14 | |||
| Drag resistance | ??41 | ??16 | ??14 | ??6 | ???11 | |||
| Refrigerant (2 minutes) | ??15 | ??25 | ??23 | ??33 | ???12 | |||
| Sliding sense (2 minutes) | ??37 | ??57 | ??42 | ??45 | ???49 | |||
| White visible deposition thing u/a | ??25 | ??7 | ??12 | ??11 | ??8 | ???51 | ||
| Thin visible deposition thing u/a | ??33 | ??6 | ??9 | ??7 | ???38 | |||
| White deposits (30 minutes) u/a | ??25 | ??8 | ??6 | ??6 | ??5 | ???40 | ||
| Thin deposit (30 minutes) u/a | ??23 | ??4 | ??3 | ??3 | ???18 | |||
| Sliding sense (30 minutes) | ??33 | ??57 | ??43 | ??43 | ???43 | |||
In embodiment 53 to 55, reuse the method that is used for embodiment 46 and prepare preparation.Described prescription is summarized in the following table 6.
Table 6
Embodiment 56 to 60
| Composition | ????53 | ????54 | ????55 |
| Wax 14 | ????15.0 | ????15.0 | ????15.0 |
| ????vol?sil?1 | ????16.8 | ????14.7 | ????12.6 |
| Oil 5 | ????4.2 | ????6.3 | ????8.4 |
| Glycerol 22 | ????10.0 | ????10.0 | ????10.0 |
| Emulsifying agent 9 | ????1.0 | ????1.0 | ????1.0 |
| ????PE?29 | ????2.0 | ????2.0 | ????2.0 |
| ????AZCH?28 | ????50.0 | ????50.0 | ????50.0 |
| Oil 30 | ????1.0 | ????1.0 | ????1.0 |
| Feature | |||
| Hardness (mm) | ????5.4 | ????8.7 | ????6.5 |
| Whiteness | |||
| Pilus Caprae seu Ovis (0h) | ????18 | ????19 | ????17 |
| Pilus Caprae seu Ovis (24h) | ????16 | ????17 | ????17 |
In embodiment 56 to 60, reuse the method that is used for embodiment 46 and prepare preparation.Described prescription is summarized in the following table 7.
Table 7
Embodiment 61 to 65
| Composition | ????56 | ????57 | ????58 | ????59 | ????60 |
| ????vol?sil?1 | ????13.05 | ????12.9 | ????13.35 | ????13.2 | ????12.9 |
| Oil 5 | ????8.7 | ????8.6 | ????8.9 | ????8.8 | ????8.6 |
| Wax 14 | ????12.5 | ????12.5 | ????12.5 | ????12.5 | ????12.5 |
| ????PE?29 | ????2.0 | ????2.0 | ????2.0 | ????2.0 | ????2.0 |
| Glycerol 22 | ????4.5 | ????4.5 | ????4.5 | ????4.5 | ????4.5 |
| Emulsifying agent 31 | ????1.25 | ????1.5 | ????--- | ????--- | ????--- |
| Emulsifying agent 32 | ????--- | ????--- | ????0.75 | ????1.0 | ????1.5 |
| ????AZCH27 | ????58.0 | ????58.0 | ????58.0 | ????58.0 | ????58.0 |
| Hardness | |||||
| Penetrate (mm) | ????9.9 | ????10.0 | ????6.7 | ????6.6 | ????7.5 |
In embodiment 61 to 65, reuse the method that is used for embodiment 46 and prepare preparation.Described prescription is summarized in the following table 8.
Table 8
Measure hardness (ball hardness) by the ball impression
| Composition | ???61 | ???62 | ????63 | ????64 | ????65 |
| ????vol?sil1 | ???12.6 | ???12.6 | ???12.6 | ???12.6 | ???12.6 |
| Oil 36 | ???8.4 | ????-- | ????-- | ????-- | ????-- |
| Oil 33 | ?????-- | ???8.4 | ????-- | ????-- | ????-- |
| Oil 34 | ?????-- | ????-- | ????8.4 | ????-- | ????-- |
| Oil 35 | ?????-- | ????-- | ????-- | ????8.4 | ????-- |
| Oil 6 | ?????-- | ????-- | ????-- | ????-- | ????8.4 |
| Emulsifying agent 9 | ????1.0 | ????1.0 | ????1.0 | ????1.0 | ????1.0 |
| ????AZCH?27 | ????58.0 | ???58.0 | ???58.0 | ???58.0 | ???58.0 |
| Water 26 | ????4.5 | ????4.5 | ????4.5 | ????4.5 | ????4.5 |
| Wax 14 | ????12.5 | ???12.5 | ???12.5 | ???12.5 | ???12.5 |
| Talcum 10 | ????2.0 | ????2.0 | ????2.0 | ????2.0 | ????2.0 |
| Oil 30 | ????1.0 | ????1.0 | ????1.0 | ????1.0 | ????1.0 |
| Hardness | |||||
| Penetrate (mm) | ????8.8 | ????6.6 | ????8.4 | ????7.5 | ????5.5 |
| Whiteness | |||||
| Pilus Caprae seu Ovis (0hr) | ????29 | ????21 | ????23 | ????17 | ????19 |
| Pilus Caprae seu Ovis (24hr) | ????68 | ????26 | ????26 | ????21 | ????16 |
The hardness of solid or soft solid can be measured by using ball to be pressed into its surface.The speed that this test set can be controlled moves ball turnover sample and measures the power that applies simultaneously.Parameter as hardness measurement is the function of maximum, force and impression place raised zones.
Concrete testing scheme uses the desk-top Instron universal testing machine (5566 type) of being furnished with 10N load chamber.Thereby the Metal Ball of diameter 9.5mm is fixed to described load chamber can be used it for and will be positioned at its below and sample on instrumented substrate is pressed and fallen into.After placing sample, the position of regulating ball is up to just on sample surfaces.Use the control software of described testing equipment to produce the continuous moving curve (subsequent motion profile) that is used for described method of testing.This curve falls into speed with the pressure of 0.05mm/s at first ball is pressed in the sample up to reaching specified power, and selected specified power makes the distance of the thrusting sample radius less than described ball.During to this load, the direction that ball moves is reversed immediately so that ball is pulled out from sample with the identical speed of 0.05mm/s.In this test process, the data of acquisition are that time (s), distance (mm) and power (N) and data acquisition speed are 25Hz.
The sample that is applicable to measurement can be loaded in the rod tube (having the screw machine device).Rod is rotated outside it protrudes the tube edge, thereby the top of using cutter to cut away tube then stays smooth uniform surface.As far as possible far rod is pushed back then in the tube and disturb at utmost to reduce any machinery from packing internal coiling machinery compliance.Twice pressure falls into each side that is pressed in spiral usually.The data that the each test of use standard spreadsheet software processes is relevant also are used to adopt following Equation for Calculating hardness H:H[N/mm
2]=F
Max[N]/A
P[mm
2] Fmax is a peak load in the formula, the protrusion area of the impression that AP keeps for the unloading back.This area can carry out geometrical calculation from the plastic indentation degree of depth and obtain.Because the strain of sample, the described plastic indentation degree of depth are lower than the overall penetration that load is measured down slightly.The plastic indentation degree of depth is calculated from the figure of unload forces to overall penetration.The initial slope of these unloading data depends on the initial elastic restoration ratio of sample.From the zero-g axle with estimate the plastic indentation degree of depth with the intercept between the straight line of the tangent of the unloading slope of corresponding plastic deformation part.Measure hardness by penetrometer
Employing is equipped with θ-wax pin, quality=2.5 grams, and the cone angle at needle point place is defined as 9 ° 10 ' ± 15 ' (ASTM D1321; IP376; DIN 51579), maximum sagging distance is 50mm laboratory equlpment PNR 10 penetrometers are measured hardness.Rod is rotated a plane, be cut into smooth uniform surface then.Pin carefully is put into the surface of rod and descended for 5 seconds with the pin (combination weight is 50 grams) of relief in its pin folder, the degree of depth that penetrates of record is measured puncture hardness so then.This method is carried out at six differences on rod surface.
Used hardness is the meansigma methods of 6 measured values.
The suitable hardness that is used for the antiperspirant materials of opening proportion container is lower than 30mm, especially is 5mm to 20mm.Sedimental measurement
Described method comprises uses reel-off gear (pay-off rig) under standard conditions AP rod sample employing equipment to be applied on the base material, and uses the average level of image analysis measurement white deposits then.I) sample is applied on the base material
Used base material is 12 * 28cm worsted wool fabric bar.
Described AP rod had not before used and had had a unaltered dome surface.
Described reel-off gear is included in every end is connected with planar substrate by clip planar substrates.Post with equipment of the standard size accepted rod tube is installed on the arm that can move along base material by air rammer control level.The spring of putting a deflection in the time of fixing described excellent makes each described rod produce identical pressure at right angle to base material.
Before test, every rod remained in the breadboard ambient temperature and spend the night.Make described rod laterally pass through base material eight times.Carefully base material is taken off and uses image analyzer directly to measure the deposit mark from described device, be i.e. the evaluation of white deposits.II) image analysis
Use angle of elevation fluorescent tube to throw light on described sample substrates to eliminate shade.Come recording picture by Sony XC77 camera with Cosmicar 16mm focal length lenses.Described camera vertically places on the reference slide and to described device and proofreaies and correct.Described sample substrates is placed under the described camera, and takes image.Use Kontron IBAS image analyzer to analyze the gained image subsequently to obtain average gray value.The whiteness that this is divided into image big cell array abstractively and measures each pixel.Measure whiteness in 0 to 255 scope, 255 for the whitest 0 being black.Suppose that low numerical value shows transparent deposit, can see the color (Lycoperdon polymorphum Vitt or black) of base material.Sense quality
By assessment panel sense quality is estimated.The appraiser relates to the assessment of the varying level of various critical sensory characteristics being carried out the modular system of example through the concordance and the sensitivity of many-sided training to guarantee their perceptual evaluations.Bao Dao sense quality is included in when applying or the refrigerant sensation after 2 minutes, white point (flakiness), drags resistance, sliding sense and thin deposit herein.Applying of product
To apply through the preparation rod product of coding measurement dosage by the appraiser with 300mg ± 30mg.Method
In test preceding 24 hours, appraiser's armpit hair is removed.All tests are implemented on the contrast test zone at least 14 appraisers.Before applying the test product, require the appraiser to adopt the not Lux of perfuming
TMFancy soap, with oxter and the forearm and the bone dry of warm water washing them.
The appraiser is applied to first kind of product their left oxter and finishes relevant score graph.The concentration and the intensity of the sense quality of each product of record on a descriptive 10cm slide-rule dial of fixing and separating.Behind the score graph of finishing left oxter, second product is applied to right oxter and repeats described method on second score graph.The appraiser is converted to mark in the 1-100 scope at the labelling on the described slide-rule dial.Calculate the various sense qualities that average mark is used for each product subsequently.When feeling under the weather, just described product is removed from their oxter appraiser's report.
Claims (36)
1. a hidroschesis activating agent, liquid-carrier and be used for the structural agent or the thickening agent of described carrier, it is characterized in that: described structural agent or thickening agent contain organic wax of the fusing point with 40 to 90 ℃, and wherein the wax of at least 60% weight satisfies formula :-CH by at least a
3-(CH
2)
n-O-CO-(CH
2)
m-CH
3Aliphatic (acid) ester provide, n is 9 to 39 in the formula, m is 0 to 35.
2. the Antipers pirant compositions of claim 1, it is characterized in that: the wax of at least 90% weight is provided by described aliphatic (acid) ester.
3. the Antipers pirant compositions of claim 1, it is characterized in that: described wax contains the free carboxy acid who is less than 2% weight.
4. the Antipers pirant compositions of claim 1, it is characterized in that: described wax contains the hydrocarbon that is less than 2% weight.
5. each Antipers pirant compositions in the aforementioned claim is characterized in that: in meeting the aliphatic (acid) ester of described general formula, n be selected from 14 to 20 and m be selected from 14 to 20.
6. the Antipers pirant compositions of claim 5, it is characterized in that: in meeting the aliphatic (acid) ester of described general formula, m is selected from 16 to 20.
7. each Antipers pirant compositions in the claim 1 to 4 is characterized in that: in meeting the aliphatic (acid) ester of described general formula, n be selected from 18 to 38 and m be selected from 0 or 1.
8. each compositions in the aforementioned claim is characterized in that: described hidroschesis activating agent comprises hydration aluminum halide, zirconium or aluminum/zirconium; Activatory hydration aluminum halide, zirconium or aluminum/zirconium; Or aluminum, zirconium or aluminum/zirconium complex or activatory aluminum, zirconium or aluminum/zirconium complex.
9. the compositions of claim 8, it is characterized in that: described hidroschesis activating agent is the complex that blended hydration zirconium chloride-aluminum, activatory aluminium chlorohydrate or aluminium chlorohydrate add zirconium and glycine, it is optional through overactivation.
10. each compositions in the aforementioned claim is characterized in that: the ratio of described hidroschesis activating agent is 5 to 40% weight.
11. each compositions in the aforementioned claim, it is characterized in that: described compositions contains volatile siloxane and optional non-volatile siloxane and/or the hydrophobic organic carrier of liquid non-silicone, and the hydrophobic organic carrier of wherein said liquid non-silicone is selected from hydrocarbon, hydrophobic aliphatic (acid) ester, aromatic ester, hydrophobic alcohol and hydrophobic ether.
12. each compositions in the aforementioned claim is characterized in that: described compositions is anhydrous composition and contains particles suspended shape hidroschesis activating agent.
13. each compositions in the claim 1 to 11 is characterized in that: described carrier contains the water that comprises the described hidroschesis activating agent of at least a portion.
14. the compositions of claim 13 is characterized in that: described compositions is an emulsion form.
15. the compositions of claim 14 is characterized in that: the decentralized photo in described emulsion accounts for 5 to 80% weight, and described continuous phase accounts for 95 to 20% weight.
16. each compositions in the claim 13 to 16 is characterized in that: described compositions contains the emulsifying agent of 0.1 to 10% weight.
17. the compositions of claim 14 is characterized in that: described continuous phase contains 10 to 35% volatile silicone oils, and 5 to 15% non-volatile hydrophobic oils,
Described decentralized photo accounts for 40 to 75%,
Described antiperspirant or deodorant activating agent account for 0.5 to 35%,
Described wax structural agent accounts for 7 to 25%,
Described emulsifying agent accounts for 0.1 to 10%,
And described compositions the highest preferred containing can reach 5% insoluble granule material,
Wherein said percent calculates based on weight.
18. the compositions of claim 17 is characterized in that: described decentralized photo accounts for 40 to 65% and preferred 45 to 60%.
19. the compositions of claim 17 or 18 is characterized in that: described compositions contains 8 to 20% and the wax structural agent of preferred 10 to 15% weight.
20. each compositions in the aforementioned claim 17 to 19 is characterized in that: described compositions contains no more than 2% C12 to C24 saturated straight chain aliphatic alcohol.
21. each compositions in the claim 17 to 20 is characterized in that: described compositions contains 10 to 20% volatile siloxane.
22. each compositions in the claim 17 to 21 is characterized in that: described nonvolatile oil is selected from 25 ℃ and is the aliphatic (acid) ester of liquid, aromatic ester and hydrocarbon down.
23. each compositions in the claim 17 to 22 is characterized in that: the volatile silicone oils that described compositions is contained and the weight ratio of nonvolatile oil are 1: 1 to 3: 1 and preferred 5: 4 to 2: 1.
24. each compositions in the claim 17 to 23 is characterized in that: described compositions contains 10 to 30% and preferred 20 to 25% water solublity hidroschesis activating agent.
25. each compositions in the aforementioned claim is characterized in that: the volatile silicone oils that described compositions is contained and the weight ratio of nonvolatile oil are 1: 1 to 3: 1 and preferred 5: 4 to 2: 1.
26. each compositions in the claim 17 to 25 is characterized in that: described compositions contains 10 to 30% and preferred 20 to 25% water solublity hidroschesis activating agent.
27. the compositions of claim 26 is characterized in that: the weight ratio of described hidroschesis activating agent and nonvolatile oil is 1: 1 to 4: 1, preferred 2: 1 to 10: 3.
28. each compositions in the claim 17 to 27 is characterized in that: described compositions contains the graininess insoluble substance of 1 to 5% weight.
29. the compositions of claim 28 is characterized in that: the contained graininess insoluble substance of described compositions is selected from Talcum, Silicon stone, clay and particulate polyethylene in small, broken bits.
30. each compositions in the claim 16 to 29 is characterized in that: described compositions contains 0.5 to 2% emulsifying agent.
31. each compositions in the claim 14 to 30 is characterized in that: described compositions also contains and reaches as high as 15%, the polyhydric alcohol of preferred 3 to 12% weight.
32. the compositions of claim 31 is characterized in that: described polyhydric alcohol is selected from glycerol and propylene glycol.
33. a method for preparing the antiperspirant rod said method comprising the steps of:
1. mix structural agent with the amount that is enough to multiviscosisty or the described carrier of structuring in the liquid-carrier and can extrude solid or solid to form, described structural agent comprises organic wax of valid density, described organic wax has 40 to 85 ℃ fusing point, and wherein the wax of at least 60% weight satisfies formula :-CH by at least a
3-(CH
2)
n-O-CO-(CH
2)
m-CH
3Aliphatic (acid) ester provide, n is 9 to 39 in the formula, m is 0 to 35,
2. make the described mixture that contains structural agent become and can flow under the high temperature,
3. described liquid-carrier is mixed with the hidroschesis activating agent, step 2 or 3 before step 1, afterwards or carry out containing the mixture of structural agent simultaneously with formation,
4. described flowable mixture is introduced in the coating container, and
The cooling or make described mixture be cooled to its multiviscosisty or structurized temperature.
34. the method for claim 33 is characterized in that: at high temperature mixed volatilization silicone oil, nonvolatile oil and wax structural agent form hydrophobic mixture; Or with described mixture heated to described structural agent fusion or dissolving or be dispersed in high temperature in the oil, formed flowable hydrophobic mixture thus,
Form simultaneously or subsequently and contain the water that water solublity or water soluble blend together branch,
In the presence of emulsifying agent,, form the emulsion that contains hydrophobic continuous phase and disperse water thus with described flowable hydrophobic mixture and water and any insoluble particulate material shear-mixed,
The cooling or make described emulsion be cooled to a certain temperature, make described continuous phase structuring form solid by described structural agent, it is characterized in that:
Described continuous phase contains 10 to 35% volatile silicone oils, 5 to 15% non-volatile hydrophobic oil,
Described decentralized photo accounts for 40 to 75%,
Described antiperspirant or deodorant activating agent account for 0.5 to 35%,
Described wax structural agent accounts for 7 to 25%,
Described emulsifying agent accounts for 0.1 to 10%,
Described compositions preferably contains and mostly is 5% insoluble granule shape material most,
Wherein said percent calculates based on the weight of described compositions.
35. one kind stops or reduces the method that human skin is perspired, described method comprises that the Antipers pirant compositions part that will contain hidroschesis activating agent, liquid-carrier and structural agent is applied on the skin, wherein said structural agent contains organic wax of the fusing point with 40 to 90 ℃, and wherein the wax of at least 60% weight satisfies formula :-CH by at least a
3-(CH
2)
n-O-CO-(CH
2)
m-CH
3Aliphatic (acid) ester provide, n is 9 to 39 in the formula, m is 0 to 35.
36. the method for claim 35 is characterized in that: the continuous phase of described compositions contains 10 to 35% volatile silicone oils, 5 to 15% non-volatile hydrophobic oils,
40 to 75% decentralized photo,
Described antiperspirant or deodorant activating agent account for 0.5 to 35%,
Described wax structural agent accounts for 7 to 25%,
Described emulsifying agent accounts for 0.1 to 10%,
And described compositions preferably contains and mostly is 5% insoluble granule shape material most,
Wherein said percent calculates based on weight.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GBGB9912924.9A GB9912924D0 (en) | 1999-06-03 | 1999-06-03 | Cosmetic compositions |
| GB9912924.9 | 1999-06-03 | ||
| GB0011084.1 | 2000-05-08 | ||
| GBGB0011084.1A GB0011084D0 (en) | 2000-05-08 | 2000-05-08 | Cosmetic compositions |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1365271A true CN1365271A (en) | 2002-08-21 |
Family
ID=26244231
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN00810971A Pending CN1365271A (en) | 1999-06-03 | 2000-06-02 | Antipers pirant compositions |
Country Status (10)
| Country | Link |
|---|---|
| US (1) | US6361765B1 (en) |
| EP (1) | EP1180010A1 (en) |
| JP (1) | JP2003501368A (en) |
| CN (1) | CN1365271A (en) |
| AU (1) | AU770263B2 (en) |
| BR (1) | BR0011256A (en) |
| CO (1) | CO5160322A1 (en) |
| MX (1) | MXPA01012368A (en) |
| PL (1) | PL204200B1 (en) |
| WO (1) | WO2000074640A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101336102B (en) * | 2006-01-27 | 2012-09-05 | 荷兰联合利华有限公司 | Antiperspirant compositions |
| CN111918634A (en) * | 2018-03-28 | 2020-11-10 | 荷兰联合利华有限公司 | Non-aluminum antiperspirant compositions |
| CN114555036A (en) * | 2019-10-16 | 2022-05-27 | 联合利华知识产权控股有限公司 | Antiperspirant compositions |
| CN114795977A (en) * | 2016-12-28 | 2022-07-29 | 施万-斯特比洛化妆品公司 | Process for producing wax products |
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| GB0002093D0 (en) * | 2000-01-28 | 2000-03-22 | Unilever Plc | Antiperspirants |
| US6534045B2 (en) | 2000-12-21 | 2003-03-18 | Colgate Palmolive Company | High efficacy antiperspirant stick |
| MXPA03005724A (en) * | 2000-12-21 | 2003-10-06 | Colgate Palmolive Co | High efficacy antiperspirant stick. |
| FR2834453B1 (en) * | 2002-01-08 | 2006-01-06 | Oreal | COMPOSITION FOR MAKE-UP OR CARE OF KERATIN MATERIALS COMPRISING A NON-VOLATILE HYDROCARBON OIL, A PARTICULAR PHASE AND A PARTICULAR DISPERSING AGENT |
| US6858666B2 (en) * | 2002-03-04 | 2005-02-22 | Aveka, Inc. | Organogel particles |
| US7347989B2 (en) * | 2003-04-01 | 2008-03-25 | The Procter & Gamble Company | High efficacy antiperspirant stick containing low levels of non-volatile organic |
| DE10317751A1 (en) * | 2003-04-17 | 2004-11-04 | Beiersdorf Ag | Anhydrous antiperspirant composition in semisolid to solid form includes a thickener system comprising hydroxyoctacosanyl 12-hydroxystearate and an inorganic and/or polymeric thickener |
| DE50305348D1 (en) * | 2003-04-24 | 2006-11-23 | Goldschmidt Gmbh | Process for the production of removable dirt and water repellent flat coatings |
| DE102004036689A1 (en) * | 2004-07-28 | 2006-03-23 | Henkel Kgaa | Low-residue deodorant or antiperspirant stick based on an oil-in-water dispersion |
| US8679464B2 (en) * | 2008-04-11 | 2014-03-25 | Kobo Products Inc. | Ternary and quaternary wax-resin composites for use in cosmetic and pharmaceutical preparations |
| JP2010037249A (en) * | 2008-08-04 | 2010-02-18 | Shiseido Co Ltd | Composite, emulsion composition containing the same and water-in-oil type emulsion cosmetic |
| US20100112022A1 (en) * | 2008-09-17 | 2010-05-06 | Jody Lynn Hoying | Antiperspirant Products and Methods of Merchandising the Same |
| US9066862B2 (en) | 2011-11-11 | 2015-06-30 | Avon Products, Inc | Self emulsified compositions |
| US20140037566A1 (en) | 2012-08-02 | 2014-02-06 | The Procter & Gamble Company | Antiperspirant Compositions and Methods |
| CA2882921C (en) | 2012-09-14 | 2017-10-24 | The Procter & Gamble Company | Aerosol antiperspirant compositions, products and methods |
| KR101470897B1 (en) * | 2013-02-08 | 2014-12-09 | 주식회사 엘지생활건강 | Cosmetic composition for deordorizing W/O emulsion |
| US9579265B2 (en) | 2014-03-13 | 2017-02-28 | The Procter & Gamble Company | Aerosol antiperspirant compositions, products and methods |
| US9662285B2 (en) | 2014-03-13 | 2017-05-30 | The Procter & Gamble Company | Aerosol antiperspirant compositions, products and methods |
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- 2000-05-31 CO CO00040642A patent/CO5160322A1/en unknown
- 2000-06-02 CN CN00810971A patent/CN1365271A/en active Pending
- 2000-06-02 JP JP2001501177A patent/JP2003501368A/en active Pending
- 2000-06-02 AU AU56776/00A patent/AU770263B2/en not_active Ceased
- 2000-06-02 PL PL352963A patent/PL204200B1/en not_active IP Right Cessation
- 2000-06-02 WO PCT/EP2000/005106 patent/WO2000074640A1/en active IP Right Grant
- 2000-06-02 EP EP00942011A patent/EP1180010A1/en not_active Ceased
- 2000-06-02 US US09/586,589 patent/US6361765B1/en not_active Expired - Lifetime
- 2000-06-02 BR BR0011256-9A patent/BR0011256A/en not_active IP Right Cessation
- 2000-06-02 MX MXPA01012368A patent/MXPA01012368A/en active IP Right Grant
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101336102B (en) * | 2006-01-27 | 2012-09-05 | 荷兰联合利华有限公司 | Antiperspirant compositions |
| CN114795977A (en) * | 2016-12-28 | 2022-07-29 | 施万-斯特比洛化妆品公司 | Process for producing wax products |
| CN111918634A (en) * | 2018-03-28 | 2020-11-10 | 荷兰联合利华有限公司 | Non-aluminum antiperspirant compositions |
| CN111918634B (en) * | 2018-03-28 | 2023-11-03 | 联合利华知识产权控股有限公司 | Non-aluminum antiperspirant compositions |
| CN114555036A (en) * | 2019-10-16 | 2022-05-27 | 联合利华知识产权控股有限公司 | Antiperspirant compositions |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1180010A1 (en) | 2002-02-20 |
| JP2003501368A (en) | 2003-01-14 |
| PL204200B1 (en) | 2009-12-31 |
| AU5677600A (en) | 2000-12-28 |
| CO5160322A1 (en) | 2002-05-30 |
| WO2000074640A8 (en) | 2003-02-20 |
| US6361765B1 (en) | 2002-03-26 |
| AU770263B2 (en) | 2004-02-19 |
| PL352963A1 (en) | 2003-09-22 |
| WO2000074640A1 (en) | 2000-12-14 |
| MXPA01012368A (en) | 2002-11-07 |
| BR0011256A (en) | 2002-03-05 |
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